CN108456139A - A kind of interval catalytic reaction rectification prepares the device and method of dibutyl phthalate - Google Patents
A kind of interval catalytic reaction rectification prepares the device and method of dibutyl phthalate Download PDFInfo
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- CN108456139A CN108456139A CN201810310004.8A CN201810310004A CN108456139A CN 108456139 A CN108456139 A CN 108456139A CN 201810310004 A CN201810310004 A CN 201810310004A CN 108456139 A CN108456139 A CN 108456139A
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- distillation column
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000066 reactive distillation Methods 0.000 claims abstract description 54
- 239000012071 phase Substances 0.000 claims abstract description 42
- 239000007791 liquid phase Substances 0.000 claims abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 238000005191 phase separation Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000008676 import Effects 0.000 claims abstract description 13
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 12
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000032050 esterification Effects 0.000 claims abstract description 12
- 238000005886 esterification reaction Methods 0.000 claims abstract description 12
- 238000002309 gasification Methods 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 239000007792 gaseous phase Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 8
- 238000007086 side reaction Methods 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 238000012856 packing Methods 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 235000019628 coolness Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- OKJADYKTJJGKDX-UHFFFAOYSA-N Butyl pentanoate Chemical compound CCCCOC(=O)CCCC OKJADYKTJJGKDX-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The present invention relates to the device and methods that a kind of interval catalytic reaction rectification prepares dibutyl phthalate.Device includes reactive distillation column, tower reactor, circulating pump, overhead condenser, tower top phase separation tank；It is characterized in that the reacted rectifying column lower part gas phase import of gas phase of the phthalic anhydride and butanol gasification in tower reactor enters in reactive distillation column, liquid phase enters the tower bottoms phase import of reactive distillation column top by circulating pump in tower reactor, and phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture of generation forms azeotropic mixture with butanol and enters split-phase in phase separation tank after overhead condenser cools down, and the butanol after split-phase is back in reactive distillation column, continues to react, and water phase is produced from split-phase pot bottom；Reactive distillation bottoms product enters in another tower reactor, is respectively equipped with catalyst bed in tower reactor and rectifying column, increases the time of esterification.Method of the present invention solves prior art seriously corroded, and side reaction is more, the more problem of waste water, and present invention process is simply controllable, the more low advantage of wastewater through organic matter content.
Description
Technical field
The invention belongs to the technical fields of catalytic reaction rectification, and in particular to a kind of adjacent benzene of interval catalytic reaction rectification preparation
The device and method of dibutyl carboxylic acid.
Background technology
Dibutyl phthalate (DBP) is a kind of good plasticizer, is current most widely used plasticizer, accounts for about
The 75% of whole plasticizer yield has very strong solvability for various kinds of resin, is mainly used for the processing of polyvinyl chloride, makes
Product softness is good；For cellulose nitrate coating, there are good emollescence and excellent stability, resistance to deflection, glues
The property, water proofing property；Also act as the plasticizer of vinyl acetate, alkyd resin, ethyl cellulose and neoprene.
Currently, domestic common synthetic method is esterified under effect of sulfuric acid with n-butanol by phthalic anhydride,
Although sulfuric acid is inexpensive, technical maturity, product yield are higher, easily cause side reaction, seriously corroded, there are three-waste pollutions and product
The shortcomings of quality is difficult to control.The master operation of DBP productions has esterification, neutralizes washing, dealcoholysis, filtering, wastewater treatment, recycles alcohol
Processing etc..Generating process generates waste water and brings water and neutralization, washing water into from chemical reaction generation water, raw materials for production.Waste water
Composition is more complicated, inside there is DBP, phthalic acid, two octanoic acid of adjacent benzene, sodium sulphate, free H2SO4, the pungent vinegar of adjacent benzene list, only son's vinegar
Equal chemical analysis give up impurities in water based on organic matter.
It is more and more urgent to the cleaning generation demand of dibutyl phthalate with the raising that Environmental Protection in China requires, it needs
The problem of being directed to traditional batch production process, a kind of DBP production technologies of efficient environmental protection are developed, improves product
Yield and conversion ratio reduce waste water yield, are all extremely important for society and enterprise.
Invention content
The present invention for the more problem of the more sewage yield of side reaction, develop a kind of environmental protection, product yield and turn
The high interval catalytic reaction rectification of rate prepares the device and method of dibutyl phthalate, to traditional esterifications reaction process into
Row improves.
Technical solution is used by the present invention solves above-mentioned technical problem：
A kind of interval catalytic reaction rectification prepares the device of dibutyl phthalate, including reactive distillation column (C1),
One tower reactor (T1), the second tower reactor (T2), circulating pump (P1), condenser (E1), phase separation tank (D)；The middle and upper part reactive distillation column (C1),
Middle part, lower part are respectively equipped with gas-liquid distributor, and catalyst sulfonate resin, the first tower reactor (T1) and are filled in gas-liquid distributor
Two tower reactors (T2) middle part, lower part are equipped with the bed of loading catalyst resin；
In reactive distillation column (C1), tower top is provided with gaseous phase outlet, and reactive distillation column (C1) tower body is from top to bottom set respectively
It is equipped with butanol refluxing opening, tower reactor fluid inlet, two tower lower part gas phase imports, bottom of tower extraction mouth；
Liquid phase entrance is provided at the top of phase separation tank (D), top is equipped with butanol bypass outlet, and bottom is equipped with water phase and produces mouth；
Gaseous phase outlet is set at the top of the first tower reactor (T1) and the second tower reactor (T2), and fluid inlet, bottom setting is arranged in top
Liquid-phase outlet；
The outlet of reactive distillation column (C1) top gaseous phase is connect with condenser (E1), condenser (E1) outlet connection phase separation tank
(D) liquid phase entrance, phase separation tank (D) upper outlet are connect with the top reactive distillation column (C1) butanol refluxing opening, reactive distillation column
(C1) gas phase entrance in lower part is connect with the first tower reactor (T1) and the second tower reactor (T2) gaseous phase outlet respectively, reactive distillation column (C1)
Bottom liquid phases outlet connect respectively with the fluid inlet of the first tower reactor (T1) and the top the second tower reactor (T2), the first tower reactor (T1) and
The outlet of second tower reactor (T2) bottom liquid phases is connect with reflux pump (P1) entrance, in reflux pump (P1) outlet and reactive distillation column (C1)
Portion's tower reactor fluid inlet connection.
A kind of method that interval catalytic reaction rectification prepares dibutyl phthalate, includes the following steps：
Reactive distillation column (C1) bottom liquid phases export with the fluid inlet on the top the first tower reactor (T1) it is separated, second
Tower reactor (T2) bottom liquid phases export it is separated with reflux pump (P1) entrance, the outlet of connection reactive distillation column (C1) bottom liquid phases with
The fluid inlet on the top the second tower reactor (T2), the outlet of connection the first tower reactor (T1) bottom liquid phases and reflux pump (P1) entrance；
Phthalic anhydride and butanol in first tower reactor (T1) are heated to 140 DEG C, phthalic anhydride：The mass ratio 1 of butanol:1.4, in catalyst
Esterification is carried out in bed；The reacted rectifying column lower part gas phase import of gas phase of first tower reactor (T1) gasification enters synthesis under normal pressure
In rectifying column (C1), in the first tower reactor (T1) liquid phase by circulating pump (P1) enter the top reactive distillation column (C1) tower bottoms mutually into
Mouthful, phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture of generation is formed altogether with butanol
It boils object and enters split-phase in phase separation tank (D) after overhead condenser (E1) is cooling, the butanol after split-phase is back to reactive distillation column (C1
It is interior), continue to react, water phase is produced from the bottom phase separation tank (D)；
Reactive distillation column (C1) bottom product enters the fluid inlet of the second tower reactor (T2), the temperature of the second tower reactor (T2)
Control is at 140 DEG C, so that mixture continuation is reacted in the catalyst bed of the second tower reactor T2, whole process is until first
Feed liquid in tower reactor T1 fully enters in reactive distillation column, the outlet of reactive distillation column (C1) bottom liquid phases and the first tower reactor (T1)
It is connected between the fluid inlet on top, the second tower reactor (T2) bottom liquid phases are exported and are connected between reflux pump (P1) entrance, instead
Answer separated, bottom the first tower reactor (T1) of the fluid inlet on the outlet of rectifying column (C1) bottom liquid phases and the top the second tower reactor (T2)
Liquid-phase outlet is separated with reflux pump (P1) entrance, and the feed liquid in the second tower reactor (T2) carries out above-mentioned anti-as reaction raw materials
Answer process, such circulate operation, until the reaction is complete.
The advantages and positive effects of the present invention are as follows：
The present invention is to replace sulfuric acid as catalyst using sulfonate resin, and reactive distillation column replaces stirred autoclave, reduces
Side reaction in reaction process, is integrated with reaction and dehydration, avoids neutralization water-washing process, the wastewater flow rate of reduction.
Method of the present invention solves prior art seriously corroded, and side reaction is more, the more problem of waste water, and
Present invention process is simply controllable, the more low advantage of wastewater through organic matter content.
Description of the drawings
Fig. 1 is the technological process that interval catalytic reaction rectification of the present invention prepares dibutyl phthalate.
C1- reactive distillation columns, E1- condensers, T1- tower reactors, T2- tower reactors, D- phase separation tanks, P1- circulating pumps, Z1- valves,
Z2- valves, Z3- valves, Z4- valves；
Liquid explanation in pipeline：1- condensate liquids, 2- reflux butanol, 3- produce water phase, 4- tower reactor liquid phases, 5- tower reactor gas
Phase, 6- tower reactor gas phases, 7- reactive distillation columns bottom of tower liquid phase, 8- reactive distillation columns bottom of tower liquid phase, 9- tower reactor liquid phases, 10- tower bottoms
Phase.
Specific implementation mode
Technical solution of the present invention is described in detail below, specific embodiment described herein is only explaining this hair
It is bright, but protection scope of the present invention is not limited to the embodiment.
Embodiment 1
Valve Z1 and Z4 are closed, and valve Z2 and Z3 are opened, phthalic anhydride and butanol in the first tower reactor T1, mass ratio 1:1.4,
It is heated to 140 DEG C in tower reactor, and carries out esterification in catalyst bed；The reacted rectifying of gas phase of first tower reactor T1 gasifications
The gas phase import of tower lower part enters in reactive distillation column C1, and liquid phase enters reactive distillation column C1 by circulating pump P1 in the first tower reactor T1
Top tower bottoms phase import, reactive distillation column rectifying tower packing be screen waviness structured packing, atmospheric operation, number of theoretical plate 12,
Phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture of generation forms azeotropic mixture with butanol
(being characterized as water content 16%, butanol amount 83%) enters split-phase in phase separation tank D, the fourth after split-phase after overhead condenser E1 coolings
In alcohol reflux to reactive distillation column C1, continue to react, water phase is produced from the bottoms phase separation tank D；It produces the bottoms reactive distillation column C1
Object enters the fluid inlet of the second tower reactor T2, and the temperature of the second tower reactor T2 is controlled at 140 DEG C, so that mixture continues in the second tower
It is reacted in the catalyst bed of kettle T2, whole process is until the feed liquid in the first tower reactor T1 fully enters reactive distillation column
In.Valve Z2 and Z3 are closed later, opens valve Z1 and Z4, and the feed liquid in the second tower reactor T2 is used as reaction raw materials, progress above-mentioned
Reaction process, such circulate operation, equipment continuous operation 2h, until the reaction is complete, finally obtained product purity are 99.7%.
Embodiment 2
Valve Z1 and Z4 are closed, and valve Z2 and Z3 are opened, phthalic anhydride and butanol in the first tower reactor T1, mass ratio 1:1.4,
It is heated to 150 DEG C in tower reactor, and carries out esterification in catalyst bed；The reacted rectifying of gas phase of first tower reactor T1 gasifications
The gas phase import of tower lower part enters in reactive distillation column C1, and liquid phase enters reactive distillation column C1 by circulating pump P1 in the first tower reactor T1
Top tower bottoms phase import, reactive distillation column rectifying tower packing be screen waviness structured packing, atmospheric operation, number of theoretical plate 12,
Phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture of generation forms azeotropic mixture with butanol
(being characterized as water content 16%, butanol amount 83%) enters split-phase in phase separation tank D, the fourth after split-phase after overhead condenser E1 coolings
In alcohol reflux to reactive distillation column C1, continue to react, water phase is produced from the bottoms phase separation tank D；It produces the bottoms reactive distillation column C1
Object enters the fluid inlet of the second tower reactor T2, and the temperature of the second tower reactor T2 is controlled at 150 DEG C, so that mixture continues in the second tower
It is reacted in the catalyst bed of kettle T2, whole process is until the feed liquid in the first tower reactor T1 fully enters reactive distillation column
In.Valve Z2 and Z3 are closed later, opens valve Z1 and Z4, and the feed liquid in the second tower reactor T2 is used as reaction raw materials, progress above-mentioned
Reaction process, such circulate operation, equipment continuous operation 2h, until the reaction is complete, finally obtained product purity are 99.8%.
Claims (2)
1. a kind of interval catalytic reaction rectification prepares the device of dibutyl phthalate, it is characterised in that：Including reactive distillation
Tower (C1), the first tower reactor (T1), the second tower reactor (T2), circulating pump (P1), condenser (E1), phase separation tank (D)；Reactive distillation column
(C1) middle and upper part, middle part, lower part are respectively equipped with gas-liquid distributor, are filled with catalyst sulfonate resin in gas-liquid distributor, and first
Tower reactor (T1) and the second tower reactor (T2) middle part, lower part are equipped with the bed of loading catalyst resin；
In reactive distillation column (C1), tower top is provided with gaseous phase outlet, and reactive distillation column (C1) tower body is from top to bottom respectively arranged with
Butanol refluxing opening, tower reactor fluid inlet, two tower lower part gas phase imports, bottom of tower produce mouth；
Liquid phase entrance is provided at the top of phase separation tank (D), top is equipped with butanol bypass outlet, and bottom is equipped with water phase and produces mouth；
Gaseous phase outlet is set at the top of the first tower reactor (T1) and the second tower reactor (T2), and fluid inlet is arranged in top, and liquid phase is arranged in bottom
Outlet；
The outlet of reactive distillation column (C1) top gaseous phase is connect with condenser (E1), condenser (E1) outlet connection phase separation tank (D) liquid
Phase entrance, phase separation tank (D) upper outlet are connect with the top reactive distillation column (C1) butanol refluxing opening, the lower part reactive distillation column (C1)
Gas phase entrance is connect with the first tower reactor (T1) and the second tower reactor (T2) gaseous phase outlet respectively, and reactive distillation column (C1) bottom liquid phases go out
Mouth is connect with the fluid inlet of the first tower reactor (T1) and the top the second tower reactor (T2) respectively, the first tower reactor (T1) and the second tower reactor
(T2) bottom liquid phases outlet is connect with reflux pump (P1) entrance, reflux pump (P1) outlet and the top reactive distillation column (C1) tower bottoms
Phase import connects.
2. a kind of method that interval catalytic reaction rectification prepares dibutyl phthalate, it is characterised in that：Include the following steps：
Reactive distillation column (C1) bottom liquid phases export with the fluid inlet on the top the first tower reactor (T1) separated, the second tower reactor
(T2) separated, connection reactive distillation column (C1) bottom liquid phases outlet and second of bottom liquid phases outlet and reflux pump (P1) entrance
The fluid inlet on the top tower reactor (T2), the outlet of connection the first tower reactor (T1) bottom liquid phases and reflux pump (P1) entrance；
Phthalic anhydride and butanol in first tower reactor (T1) are heated to 140 DEG C, phthalic anhydride：The mass ratio 1 of butanol:1.4, in catalyst bed
Middle carry out esterification；The reacted rectifying column lower part gas phase import of gas phase of first tower reactor (T1) gasification enters synthesis under normal pressure rectifying
In tower (C1), liquid phase enters the top reactive distillation column (C1) tower bottoms phase import, benzene by circulating pump (P1) in the first tower reactor (T1)
Acid anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture of generation forms azeotropic mixture warp with butanol
Entering split-phase in phase separation tank (D) after overhead condenser (E1) is cooling, the butanol after split-phase is back to reactive distillation column (in C1), after
Continuous to be reacted, water phase is produced from the bottom phase separation tank (D)；
Reactive distillation column (C1) bottom product enters the fluid inlet of the second tower reactor (T2), and the temperature control of the second tower reactor (T2) exists
140 DEG C, so that mixture continuation is reacted in the catalyst bed of the second tower reactor T2, whole process is until the first tower reactor T1
In feed liquid fully enter in reactive distillation column, the outlet of reactive distillation column (C1) bottom liquid phases and the liquid on the top the first tower reactor (T1)
It is connected between phase import, the second tower reactor (T2) bottom liquid phases are exported and are connected between reflux pump (P1) entrance, reactive distillation column
(C1) fluid inlet of bottom liquid phases outlet and the top the second tower reactor (T2) is separated, the outlet of the first tower reactor (T1) bottom liquid phases
Separated with reflux pump (P1) entrance, the feed liquid in the second tower reactor (T2) carries out above-mentioned reaction process, such as reaction raw materials
This circulate operation, until the reaction is complete.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810310004.8A CN108456139B (en) | 2018-04-09 | 2018-04-09 | Device and method for preparing dibutyl phthalate by batch catalytic reaction rectification |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810310004.8A CN108456139B (en) | 2018-04-09 | 2018-04-09 | Device and method for preparing dibutyl phthalate by batch catalytic reaction rectification |
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| CN108456139B CN108456139B (en) | 2024-01-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111960943A (en) * | 2020-08-27 | 2020-11-20 | 江苏正丹化学工业股份有限公司 | Process for producing dioctyl terephthalate by semi-continuous method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106810450A (en) * | 2017-02-23 | 2017-06-09 | 天津大学 | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate |
| US20170267615A1 (en) * | 2014-06-05 | 2017-09-21 | Shanghai Wuzheng Engineering Technology Co., Ltd | Method and device system for producing dimethyl oxalate through midhigh and high-pressure carbonylation of industrial synthesis gas and producing ethylene glycol through dimethyl oxalate hydrogenation |
| CN208166890U (en) * | 2018-04-09 | 2018-11-30 | 石家庄白龙化工股份有限公司 | Interval catalytic reaction rectification prepares the device of dibutyl phthalate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170267615A1 (en) * | 2014-06-05 | 2017-09-21 | Shanghai Wuzheng Engineering Technology Co., Ltd | Method and device system for producing dimethyl oxalate through midhigh and high-pressure carbonylation of industrial synthesis gas and producing ethylene glycol through dimethyl oxalate hydrogenation |
| CN106810450A (en) * | 2017-02-23 | 2017-06-09 | 天津大学 | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate |
| CN208166890U (en) * | 2018-04-09 | 2018-11-30 | 石家庄白龙化工股份有限公司 | Interval catalytic reaction rectification prepares the device of dibutyl phthalate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111960943A (en) * | 2020-08-27 | 2020-11-20 | 江苏正丹化学工业股份有限公司 | Process for producing dioctyl terephthalate by semi-continuous method |
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